CN104151836A - Heat-conducting silicone grease and preparation method thereof - Google Patents
Heat-conducting silicone grease and preparation method thereof Download PDFInfo
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Abstract
The invention relates to heat-conducting silicone grease and a preparation method thereof, and aims at improving the heat-conducting performance, electrical insulation performance and weather resistance of the heat-conducting silicone grease. The heat-conducting silicone grease comprises the following components in parts by weight: 70-80 parts of nano diamond, 5-10 parts of a phase change capsule, 10-20 parts of resin and 10-20 parts of silicone oil. The preparation method comprises the following steps: uniformly mixing the components in parts by volume at the speed of 2,500-3,500rpm to obtain a mixture; vacuumizing the mixture in a vacuum mixer for 1.5-3 hours to obtain the heat-conducting silicone grease. According to the preparation method, the nano diamond and the phase change capsule are added, so that the heat-conducting coefficient of the silicone grease is increased, the temperature resistance of the silicone grease is improved, the bonding gap between interfaces is reduced, and the heat-conducting silicone grease has a phase change effect, high heat-conducting property and good electrical insulation property and weather resistance in use.
Description
Technical field
The present invention relates to heat interfacial material field, is a kind of heat-conducting silicone grease and preparation method thereof specifically.
Background technology
Increasingly mature along with the guiding of national policy and chip technology, it is also popular that energy-efficient semiconductor LED light fixture replaces traditional energy-saving lamp, high-pressure mercury lamp, tengsten lamp starts commercialization, more and more enter common people house, but at present LED chip technology only has 30% electric energy to be converted to light, other 70% electric energy is converted to heat, LED semiconductor die package becomes light source and uses as light fixture, if can not effectively dissipate these heats, consequent heat effect will cause junction temperature to raise, the photon that directly reduces chip outgoing, reduces and gets optical efficiency.The rising of temperature also can make the emmission spectrum generation red shift of chip, makes colour temperature Quality Down, especially even more serious to excite the white light LED part of yellow fluorescent powder based on blue-ray LED, and wherein the efficiency of conversion of fluorescent material also can be along with temperature raises and reduces.Simultaneously, in the course of the work due to chip repeat heating, power model is the effect of experience thermal cycling load constantly, because the thermal expansivity (CTE) of differing materials does not mate, can produce interlayer thermal stresses, and As time goes on can there is warpage, peel off, crackle, even produce and lost efficacy and dead lamp, this is also a major cause that causes LED and power model ultimate failure.Therefore, because the temperature various heat effect that produce that raise are gathered work-ing life and the reliability that can badly influence LED light fixture.
And as 21 century the robot arm produced of intelligentized robot, automatic industrial, computer system core the arithmetic speed of central processor CPU more and more faster, its thermal value also increases thereupon.If CPU heat radiation is bad, excess Temperature, is easy to cause intelligent equipment in operational process, to occur the problems such as equipment interruption suddenly, warm start, deadlock.Therefore, for CPU provides good passage of heat, and ensureing that by heat-removal system equipment moves automatically, intelligent control, is one of essential condition of the normal work of computer.
For the heat dissipation problem of the pyrotoxins such as high-power LED lighting system thermal source and cpu chip, conventional method is that radiator element is installed on pyrotoxin.Even and also inevitably there is a fixed gap in very smooth face-face contact between the thermals source such as CPU and radiator element, the existence in space will seriously affect heat-conducting effect, thereby affect the radiating effect of final scatterer, finally affect product stability and reliability.
Heat interfacial material is used widely because can effectively reduce the interface resistance between thermal source and scatterer.Heat-conducting silicone grease is exactly a kind of the most conventional heat-conducting medium wherein, it is the material for filling space between pyrotoxin and radiator element, the heat that thermal source is come out conducts to radiator element, make heat source temperature remain on one can steady operation level, in the work-ing life that extends device, prevent that thermal source is bad and impaired because dispelling the heat.
Heat-conducting silicone grease is that heat conduction stopping composition adds resin, silicone oil mixes, the common two large classes that are mainly divided in market a: class is the most common white heat-conducting silicone grease, this class heat-conducting silicone grease is the liquid state of thickness at normal temperatures, and its filler is mainly aluminum oxide, boron nitride, silicon carbide, aluminium powder; Another kind of is grey heat-conducting silicone grease.This class heat-conducting silicone grease is in white conduction estersil, to have added a certain amount of graphite, and to strengthen its heat conductivility, the filler of grey heat-conducting silicone grease is generally graphite, silver powder or high thermal conductivity nano-metal-oxide.
In existing high-end heat-conducting silicone grease, additive is generally silver powder and graphite material, the thermal conductivity of Graphite Powder 99 is generally at 200-300W/ (MK), the thermal conductivity of silver powder is only also 429W/ (MK), and expensive, helps limited to the raising of silicone grease bulk thermal conductivity, and because simple metal is filled, easily conduction, will cause LED light fixture and CPU electric leakage and safety problem, and impact is used safety.
In addition, in life-time service process, often there is the phenomenon that silicone oil separates with heat conductive filler, cause the sclerosis of existing heat-conducting silicone grease ubiquity coating, efflorescence, cracked, the problems such as heat conductivility variation.
Summary of the invention
Technical problem to be solved by this invention is to provide heat-conducting silicone grease of a kind of good heat conductivity and preparation method thereof.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of heat-conducting silicone grease, comprises the component of following weight part:
Heat-conducting silicone grease of the present invention, has following beneficial effect:
By the interpolation of nanometer diamond material and phase transformation capsule, not only improve the thermal conductivity of silicone grease itself, and improve the heat resistance of silicone grease itself and reduce the bonding gap between interface, make heat-conducting silicone grease there is phase transformation effect, high thermal conductivity, there is good electric insulating quality simultaneously and use weather resistance, having solved traditional silicone grease in use because of problems such as the heat-conducting effect that excess Temperature occurs is poor, conduction, easily sclerosis, efflorescence.Adopt heat-conducting silicone grease of the present invention, can greatly improve the processing power of thermal source heat passage, reduce the internal stress between material of gathering of hot-fluid, reduce interface temperature and thermal resistance between thermal source and scatterer, improve job stability and the work-ing life of thermal source.
In order to solve the problems of the technologies described above, the present invention also provides a kind of preparation method of above-mentioned heat-conducting silicone grease, comprises the following steps:
By the component mixing and stirring of each weight part, stirring velocity is 2500～3500rpm;
The material obtaining after stirring is placed in vacuum mixer and vacuumizes and process 1.5～3h, obtain heat-conducting silicone grease.
Preparation method of the present invention, has following beneficial effect:
1, by the interpolation of nanometer diamond material and phase transformation capsule, not only improve the thermal conductivity of silicone grease itself, and improve the heat resistance of silicone grease itself and reduce the bonding gap between interface, make heat-conducting silicone grease there is phase transformation effect, high thermal conductivity, there is good electric insulating quality simultaneously and use weather resistance, having solved traditional silicone grease in use because of problems such as the heat-conducting effect that excess Temperature occurs is poor, conduction, easily sclerosis, efflorescence.
2, the present invention adopts the mode of high-speed stirring to mix each component, and then mixed material is passed through to the centrifugal vacuum defoamation of vacuum mixer, eliminate the bubble of material the inside, prevent that the existence of bubble from reducing the heat-conducting effect of heat-conducting silicone grease, effectively improved the thermal conductivity of silicone grease, whole technique is simple to operation.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, be explained in detail below in conjunction with embodiment.
The design of most critical of the present invention is: high thermal conductivity and the high insulating property of utilizing nanometer diamond, and good wetting property and the phase-change characteristic of phase transformation capsule, make heat-conducting silicone grease there is phase transformation effect, high thermal conductivity, there is good electric insulating quality simultaneously and use weather resistance, having solved traditional silicone grease in use because of problems such as the heat-conducting effect that excess Temperature occurs is poor, conduction, easily sclerosis, efflorescence.
Concrete, the heat-conducting silicone grease of the embodiment of the present invention, comprises the component of following weight part:
The thermal conductivity of diamond is 2300W/ (MK), far above the thermal conductivity of Graphite Powder 99 and silver powder, and itself have high-insulation effect, insulation effect is consistent with stupalith, as the application of the interpolation composition aspect of heat-conducting silicone grease, have not yet to see report.
Adopting phase transformation capsule to do coordinates, with nanometer diamond, resin, after silicone oil and additive mix, itself and thermal source are (as LED, CPU), between scatterer, there is good wetting property at interface, when particularly temperature reaches transformation temperature, its phase transformation component substances is from the solid-state liquid state that becomes, just can better infiltrate the gap between interface, thermally conductive material in heat-conducting silicone grease (nanometer diamond) is disperseed uniformly, the inside, interface air is extruded, and reduce the sclerosis of its material powder, efflorescence, cracked possibility, thereby reduce the thermal contact resistance between thermal source and scatterer interface, improve heat conductivility.
Therefore, the present invention is by adding nanometer diamond and phase transformation capsule, and rational allocation nanometer diamond, phase transformation capsule, resin, silicone oil and the content of additive in heat-conducting silicone grease, not only improve the thermal conductivity of silicone grease itself, and improved electrical insulation properties and the weather resistance of silicone grease itself.After tested, the thermal conductivity value of heat-conducting silicone grease of the present invention can reach 8.0～9.0W/ (MK), during as light source thermally conductive material, the temperature difference of light source and scatterer is between 2～3 DEG C, through not efflorescence after 230 DEG C, the continuous heat treatment of 5000h, not cracked, do not become dry, still be the thickness state of plasticine, and thermal conductivity value conservation rate >=97%.
From foregoing description, beneficial effect of the present invention is:
By the interpolation of nanometer diamond material and phase transformation capsule, not only improve the thermal conductivity of silicone grease itself, and improve the heat resistance of silicone grease itself and reduce the bonding gap between interface, make heat-conducting silicone grease there is phase transformation effect, high thermal conductivity, there is good electric insulating quality simultaneously and use weather resistance, having solved traditional silicone grease in use because of problems such as the heat-conducting effect that excess Temperature occurs is poor, conduction, easily sclerosis, efflorescence.Adopt heat-conducting silicone grease of the present invention, can greatly improve the processing power of thermal source heat passage, reduce the internal stress between material of gathering of hot-fluid, reduce interface temperature and thermal resistance between thermal source and scatterer, improve job stability and the work-ing life of thermal source.
In the above-described embodiments, described nanometer diamond can be grown by vapour deposition process, as pass through ICP, PECVD, the semiconductor manufacturing equipment deposition growings such as MOCVD, its granularity D50 is preferably 10-100nm, thermal conductivity is 2300W/ (MK), nanometer diamond surface can further possess lipophilicity and hydrophobicity after treatment, to prevent that the intervention of atmospheric vapour from causing silicone grease to use rear material surface and internal oxidation, concrete treatment process can be with reference to as described below: nanometer diamond is added to paraffin wax emulsions, fully mix, make paraffin form hydrophobic integument on powder (nanometer diamond) surface.Nanometer diamond thermal expansivity is little, and internal stress is little, good stability, and high-insulation, specific refractory power is high, can not cause light-source brightness loss.
In the above-described embodiments, described phase transformation capsule is inorganic metal or its oxide compound of parcel paraffin, itself has high heat conduction, high insulation effect, and Main Function is its phase transformation effect.Preferably, described inorganic metal or its oxide compound are selected from one or more in aluminium nitride, titanium oxide, magnesium oxide, aluminum oxide and zinc oxide, and its capsule grain is through between 30-80 μ m.Like this in the time that thermal source (as light source or CPU) temperature is elevated to more than 50 DEG C, silicone grease will be by the thick solid-state fluid liquid state that is converted to of height, reach rapidly and disperse silicone grease and nanometer diamond composition, increase surface-area, form a film and fill the gap between thermal source and scatterer, and follow the rising of temperature, between its thermal source, interface effect of impregnation is strengthened, interfacial gap and thermally conductive pathways diminish, thereby reach the effect that reduces junction temperature and reduce thermal resistance.
In the above-described embodiments, described resin can adopt the resin using in existing heat-conducting silicone grease, preferably, the present invention adopts the liquid silicone resin of the active group that contains hydroxyl and/or vinyl, the described liquid silicone resin that contains hydroxyl as DOW CORNING 233 (common name: flaky resin, trade name/trade mark:
rSN-0233, chemical Chinese: hydroxy functional group silicone resin, chemical English name: Hydroxyl-functional Silicone Resin, supplier: DOW CORNING/XIAMETER); The described liquid silicone resin that contains vinyl is as methyl vinyl MQ high viscosity resins (M/Q ratio: 0.8, product type: AM ?8071, supplier: Guangzhou Xin Hou Chemical Industry Science Co., Ltd).The particle diameter D50 of described resin is preferably 0.1～10.0 μ m, and the viscosity at 25 DEG C is preferably 20000～250000cSt, and purity is preferably more than 99.8%.
In the above-described embodiments, described silicone oil can adopt the silicone oil using in existing heat-conducting silicone grease, preferably, it is the micromolecular activated silica oil cpd of 5.0～50.0cSt (25 DEG C) that the present invention adopts viscosity, such as one or more in hydroxy silicon oil, containing hydrogen silicone oil, methoxyl group silicone oil and vinyl silicone oil, by the high purity product of chemical distillation gained.
In the above-described embodiments, described heat-conducting silicone grease can also comprise other additive components such as optional fire retardant, stablizer, thixotropic agent, catalyzer, and the amount of additive is preferably 0.5-1 weight part.
Specific embodiment 1
1, material composition and metering formula
2, preparation method
Take material: take by above-mentioned material metering formula, be placed in the stirrer still of 5L;
Evenly mix: be stirred to evenly with homogenizer, stirring velocity is 3000rpm, is mobile paste body shape;
Vacuum outgas: carry out in vacuum mixer, vacuumize and process 2h, obtain heat-conducting silicone grease.
3, test result
After testing, the thermal conductivity value of gained heat-conducting silicone grease is 8.0W/ (MK), and through 230 DEG C, the continuous heat treatment of 5000h, result shows the not efflorescence of heat-conducting silicone grease coating, not cracked, does not become dry, and is still the thickness state of plasticine.After Overheating Treatment, recording its thermal conductivity value is 7.9W/ (MK), and conservation rate is 96.7%.
Specific embodiment 2
1, material composition and metering formula
2, preparation method
Take material: take by above-mentioned material metering formula, be placed in the stirrer still of 5L;
Evenly mix: be stirred to evenly with homogenizer, stirring velocity is 3000rpm, is mobile paste body shape;
Vacuum outgas: carry out in vacuum mixer, vacuumize and process 2h, obtain heat-conducting silicone grease.
3, test result
After testing, the thermal conductivity value of gained heat-conducting silicone grease is 8.5W/ (MK), and through 230 DEG C, the continuous heat treatment of 5000h, result shows the not efflorescence of heat-conducting silicone grease coating, not cracked, does not become dry, and is still the thickness state of plasticine.After Overheating Treatment, recording its thermal conductivity value is 8.5W/ (MK), and conservation rate is 100%.
Specific embodiment 3
1, material composition and metering formula
2, preparation method
Take material: take by above-mentioned material metering formula, be placed in the stirrer still of 5L;
Evenly mix: be stirred to evenly with homogenizer, stirring velocity is 3000rpm, is mobile paste body shape;
Vacuum outgas: carry out in vacuum mixer, vacuumize and process 2h, obtain heat-conducting silicone grease.
3, test result
After testing, the thermal conductivity value of gained heat-conducting silicone grease is 8.3W/ (MK), and through 230 DEG C, the continuous heat treatment of 5000h, result shows the not efflorescence of heat-conducting silicone grease coating, not cracked, does not become dry, and is still the thickness state of plasticine.After Overheating Treatment, recording its thermal conductivity value is 8.1W/ (MK), and conservation rate is 98%.
The heat-conducting silicone grease (code name is respectively 001,002,003) that above-mentioned specific embodiment 1-3 is prepared, and the heat-conducting silicone grease (code name is TC) that Dow Corning Corporation produces carries out light source temperature rise test as light source thermally conductive material respectively.Wherein, the LED integrated optical source that light source is 50W, scatterer is the scatterer of 50W same size, after energising test its light at interval of 1H light source substrate temperature and radiator temperature, light continuously after it reaches thermal equilibrium 8H temperature test data as shown in the table:
Known by above table data, when heat-conducting silicone grease of the present invention is used as light source thermally conductive material, the temperature difference of light source and scatterer is between 2-3 DEG C, and the temperature difference of TC is between 6-7 DEG C, illustrates that the heat-conducting effect of the heat-conducting silicone grease of the present invention that adds nanometer diamond and phase transformation capsule is better than common silicone grease.
In sum, the heat-conducting silicone grease of dopen Nano diamond and phase transformation capsule, as outstanding heat interfacial material, thermal conductivity value reaches 8.0～9.0W/ (MK), and little by difference variation between actual measurement light source and scatterer, there is high thermal conductivity, there is good use weather resistance simultaneously, not efflorescence of heat-conducting silicone grease coating in long use procedure, not cracked, do not become dry, remain the thickness state of plasticine, and heat conductivility is substantially constant, thermal conductivity coefficient value conservation rate >=97%.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention to do, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. a heat-conducting silicone grease, is characterized in that, comprises the component of following weight part:
2. heat-conducting silicone grease according to claim 1, is characterized in that: the granularity D50 of described nanometer diamond is 10-100nm, and thermal conductivity is 2300W/ (MK).
3. heat-conducting silicone grease according to claim 1, is characterized in that: described nanometer diamond is that surface has lipophilicity and hydrophobic nanometer diamond.
4. heat-conducting silicone grease according to claim 1, it is characterized in that: described phase transformation capsule is inorganic metal or its oxide compound of parcel paraffin, and described inorganic metal or its oxide compound are selected from one or more in aluminium nitride, titanium oxide, magnesium oxide, aluminum oxide and zinc oxide.
5. heat-conducting silicone grease according to claim 1, is characterized in that: the particle diameter of described phase transformation capsule is 30-80 μ m.
6. heat-conducting silicone grease according to claim 1, is characterized in that: described resin is the liquid silicone resin of the active group that contains hydroxyl and/or vinyl.
7. heat-conducting silicone grease according to claim 1, is characterized in that: the particle diameter D50 of described resin is 0.1～10.0 μ m, and the viscosity at 25 DEG C is 20000～250000cSt, and purity is 99.8%.
8. heat-conducting silicone grease according to claim 1, is characterized in that: described silicone oil is selected from one or more in hydroxy silicon oil, containing hydrogen silicone oil, methoxyl group silicone oil and vinyl silicone oil, and the viscosity at 25 DEG C is 5.0～50.0cSt.
9. heat-conducting silicone grease according to claim 1, is characterized in that: also comprise the additive of 0.5-1 weight part, described additive is selected from one or more in fire retardant, stablizer, thixotropic agent and catalyzer.
10. a preparation method for the heat-conducting silicone grease as described in claim 1-9 any one, is characterized in that, comprises the following steps:
By the component mixing and stirring of each weight part, stirring velocity is 2500～3500rpm;
The material obtaining after stirring is placed in vacuum mixer and vacuumizes and process 1.5～3h, obtain heat-conducting silicone grease.
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| CN104531053A (en) * | 2014-12-18 | 2015-04-22 | 深圳新宙邦科技股份有限公司 | Solid crystal gel for LED as well as preparation method and application of solid crystal gel |
| CN109844030A (en) * | 2016-10-18 | 2019-06-04 | 信越化学工业株式会社 | Heat-conductive silicone composition |
| CN114181532A (en) * | 2021-12-22 | 2022-03-15 | 仲恺农业工程学院 | Phase-change heat-conducting silicone grease containing macromolecular modifier and preparation method thereof |
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| CN104531053A (en) * | 2014-12-18 | 2015-04-22 | 深圳新宙邦科技股份有限公司 | Solid crystal gel for LED as well as preparation method and application of solid crystal gel |
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